Composition for controlling soil pests, containing, as active ingredient, glucosinolate extracted from rapeseed meal and eutrema japonicum, and preparation method therefor

Abstract

A composition for controlling soil pests, containing, as an active ingredient, glucosinolate extracted from rapeseed meal and Eutrema japonicum, of the present invention, is obtained by performing extraction on dried rapeseed meal powder in ethanol and water as solvents at an extraction temperature of room temperature to 70°C for 30 minutes to three days so as to extract progoitrin, gluconapin and 4-hyroxyglucobrassicin, which are indicator ingredients, and performing extraction on dried Eutrema japonicum sample in ethanol and water at an extraction temperature of room temperature to 70°C for 30 minutes to three days so as to extract sinigrin, which is an indicator ingredient, thereby mixing the two extracted ingredients.

Description

A composition for controlling soil pests having glucosinolates extracted from rapeseed meal and horseradish as an active ingredient, and a method for manufacturing the same

[0001] The present invention relates to a composition for controlling soil pests containing glucosinolates extracted from rapeseed meal and horseradish as an active ingredient, and a method for manufacturing the same. More specifically, the invention relates to a composition of natural origin with excellent efficacy in controlling soil pests, which effectively provides a composition of natural origin with low acute toxicity to fish and honeybees, and is an eco-friendly material containing glucosinolates extracted from rapeseed meal and horseradish as an active ingredient that is safe for the human body and contains within levels safe for humans, and is free from acute oral and acute dermal toxicity, eye mucosal and skin irritation compared to chemical pesticides, and a method for manufacturing the same.

[0002] Plant-parasitic nematodes are pests that cause massive damage to crops by occurring in large numbers in soils of continuous cropping sites, resulting in trillions of dollars in losses worldwide every year. These plant-parasitic nematodes, belonging to the phylum Platyhelminthes, number in the thousands of species and, depending on their feeding method, morphology, and parasitic behavior, include root-knot nematodes (Meloidogyne spp.), root-rotting nematodes (Paratylenchus spp.), dwarf nematodes (Tylenchorhynchus spp.), needle nematodes (Paratylenchus spp.), ring nematodes (Criconemoides spp.), spiral nematodes (Hellicotylenchus spp.), cyst nematodes (Heterodera spp.), stem nematodes (Ditylenchus spp.), and leaf nematodes (Aphelenchoides spp.).

[0003] In domestic greenhouse horticulture sites, infection by root-knot nematodes causes an annual yield reduction of approximately 30-40%, and these nematodes damage almost all greenhouse horticultural crops in Korea, including cucumbers, watermelons, Korean melons, and tomatoes. These root-knot nematodes (Meloidogyne spp.) were first discovered in the 1850s in cucumber root galls grown in greenhouses in England, and were established as the genus Meloidogyne sp. by Chitwood in 1949, with 78 species distributed worldwide. In Korea, peanut root-knot nematodes (Meloidogyne arenaria), carrot root-knot nematodes (Meloidogyne hapla), sweet potato root-knot nematodes (Meloidogyne incognita), and Javanica root-knot nematodes are being studied. These are the most difficult-to-control and damaging nematodes that cause damage to fruit and vegetable crops such as Korean melons, cucumbers, tomatoes, strawberries, chili peppers, and watermelons, as well as ginseng.

[0004] To address the nematode problem causing significant damage to such greenhouse cultivation sites, various nematode control agents have been researched and marketed. However, as the adverse effects of conventional synthetic organic pesticides on the human body and the natural environment have been revealed, their use has been avoided. Consequently, various natural control agents have been researched and proposed to replace them. For example, Korean Patent Publication No. 2017-0124329 (Patent Document 1) discloses a "composition for nematode control containing geraniol," which describes "a composition for nematode control characterized by containing geraniol at a concentration of 200 to 3,000 ppm and possessing nematicidal activity against root-knot nematodes, root-rot nematodes, spiral nematodes, and cistern nematodes without causing phytotoxicity to host plants." Additionally, Korean Patent Publication No. 2020-0109850 (Patent Document 2) describes a "method for controlling root-knot nematode disease using a mixture of maleic acid and copper sulfate." "Disclosing a nematicid composition comprising maleic acid and copper sulfate, wherein the concentration of maleic acid is 0.01 to 10 mmol / L and the concentration of copper sulfate is 0.01 to 10 mmol / L."

[0005] In addition, Korean Patent Registration No. 102313198 (Patent Document 3) discloses a "nematicidal composition against Meloidogyne nematodes comprising a culture filtrate of Lactobacillus plantarum WiKim0090 (accession number KFCC11865P) or a concentrate of said culture filtrate as an active ingredient" under the title "Method for controlling root-knot nematodes using Lactobacillus plantarum WiKim0090", and Korean Patent Registration No. 101771962 (Patent Document 4) discloses a "nematode control composition comprising a mixed preparation of rapeseed cake and mustard cake as an active ingredient, wherein rapeseed cake and mustard cake are mixed in a weight ratio of 5:1 to 1:5" under the title "Composition for controlling nematodes comprising a mixed preparation of rapeseed cake and mustard cake as an active ingredient."

[0006] However, although the nematode control compositions disclosed in the aforementioned conventional patent literature are environmentally friendly products derived from nature, there was still room for improvement in their control efficacy. In particular, there is a demand for a soil pest control agent that can be easily utilized by farmers suffering from increased pests due to the global subtropicalization, thereby providing an effective soil pest control agent to organic farms where chemical pesticides are prohibited, which not only prevents crop damage but also reduces labor costs.

[0007] Accordingly, the inventors recognized the problems in the aforementioned conventional technology and, as a result of diligent research to solve them, analyzed the control-effective components of rapeseed meal and / or horseradish, which have been used as raw materials for natural nematode control agents in order to improve control efficacy. By effectively extracting the control-effective components identified therefrom, such as progoitrin, gluconapin, 4-hydroxyglucobrassicin, and sinigrin, which are types of glucosinolates, and providing them as natural nematode control agents, they discovered that a composition and a method for manufacturing the same can effectively solve the problems in the aforementioned conventional technology, thereby completing the present invention.

[0008] (Prior Art Literature)

[0009] (Patent Document 1) Patent Document 1: Republic of Korea Patent Publication No. 2017-0124329

[0010] (Patent Document 2) Patent Document 2: Korean Patent Publication No. 2020-0109850

[0011] (Patent Document 3) Patent Document 3: Republic of Korea Patent Registration No. 102313198

[0012] (Patent Document 4) Patent Document 4: Republic of Korea Patent Registration No. 101771962

[0013] Accordingly, the present invention has been made in consideration of the technical problems in the aforementioned prior art. The main objective of the present invention is to provide a composition for controlling soil pests containing glucosinolate extracted from rapeseed cake and horseradish as an active ingredient, which enables optimal control of root-knot nematodes in field crops by effectively extracting glucosinolate, an active ingredient for control, from rapeseed cake and horseradish, which have been used as raw materials for natural nematode control agents in the past, in order to improve the control efficacy of these materials.

[0014] Another objective of the present invention is to provide a composition for controlling soil pests that enables labor reduction through formulation research of a nematode control agent having the specific efficacy described above.

[0015] Another objective of the present invention is to provide a method for more efficiently producing a soil pest control composition having glucosinolates extracted from rapeseed meal and horseradish as an active ingredient, which achieves the specific purpose mentioned above.

[0016] The inventors, after careful consideration to achieve the above objective, discovered that soil pests can be effectively controlled by effectively extracting glucosinolate-based components, which are the main components of pest control efficacy, from rapeseed cake and horseradish using ethanol and water, thereby completing the present invention.

[0017] Accordingly, the soil pest control composition of the present invention, comprising glucosinolates extracted from rapeseed meal and horseradish as an active ingredient to achieve the above objective, comprises:

[0018] The invention is characterized by being obtained by mixing two extracted components, wherein dried rapeseed meal powder is extracted by performing extraction in ethanol and water at a temperature of room temperature to 70°C for 30 minutes to 3 days to extract the indicator components progoitrin, gluconapin, and 4-hydroxyglucobrassicin, and dried horseradish sample is extracted by performing extraction in ethanol and water at a temperature of room temperature to 70°C for 30 minutes to 3 days to extract the indicator component sinigrin.

[0019] According to another configuration of the present invention, the extract component is characterized by being a diluted solution composition diluted 10 times with zeolite.

[0020] According to another configuration of the present invention, the solvents ethanol and water are characterized by using 60% ethanol in a ratio of 10 to 40 when used with dried rapeseed meal powder, and using 60% ethanol in a ratio of 10 to 40 when used with dried horseradish samples.

[0021] In addition, the method for preparing a soil pest control composition according to the present invention, comprising glucosinolates extracted from rapeseed meal and horseradish as an active ingredient to achieve the other objectives mentioned above, comprises:

[0022] Step of grinding dried rapeseed meal powder:

[0023] A step of performing stirring extraction or reflux extraction using the ground material as a solvent in 10 to 40 times 60% ethanol at room temperature to 70°C for 30 minutes to 3 days:

[0024] A step of filtering the above extract and performing continuous centrifugation;

[0025] Step of removing alcohol and water by concentrating the centrifuged material under reduced pressure: and

[0026] A step of freeze-drying the extract;

[0027] Step of freeze-drying a dried horseradish sample;

[0028] Step of grinding the freeze-dried sample;

[0029] Step of performing reflux extraction of the ground sample using 60% ethanol as a solvent in 10 to 40 times the amount at room temperature to 70°C for 30 minutes to 3 days:

[0030] A step of performing continuous centrifugation on the above extract;

[0031] Step of removing alcohol and water by concentrating the centrifuged material under reduced pressure: and

[0032] It consists of a freeze-drying step of the extract,

[0033] It is characterized by comprising the step of mixing each of the above freeze-dried extracts in a fixed ratio.

[0034] According to another configuration of the present invention, the mixing ratio of the freeze-dried extract of rapeseed meal and horseradish is characterized by being mixed in a weight ratio of 1:5 to 5:1.

[0035] The soil pest control composition comprising glucosinolates extracted from rapeseed meal and horseradish as active ingredients according to the present invention, and the method for manufacturing the same, configured as described above, effectively provide a naturally derived composition with excellent efficacy in controlling soil pests. This composition is an eco-friendly material that is safe for the human body, containing levels within which it exhibits acute oral and dermal low toxicity compared to chemical pesticides, and is free from irritation to the eye mucosa and skin. By utilizing glucosinolates, which are active ingredients extracted from rapeseed meal and horseradish, it is possible to produce and provide a high-content organic compound fertilizer for soil nematode control. Furthermore, since this can be manufactured in various formulations, labor savings can be maximized through changes in formulation. While the nematode control effect is low when plant extracts are sprayed onto the soil in liquid form, applying the plant extract of the present invention to the soil in the form of granule pellets—formed by adsorbing the extract onto zeolite and mixing it with plant oilseed meal—allows for the uniform distribution of active ingredients, thereby further enhancing the control effect against soil pests and root-knot nematodes. Additionally, the release rate can be controlled, and spraying It also provides a useful functional effect that solves all the problems required in the aforementioned conventional technology by making it convenient and increasing effectiveness.

[0036] FIG. 1 is a diagram showing a process for extracting an active ingredient from rapeseed meal to prepare a soil pest control composition having glucosinolate extracted from rapeseed meal and horseradish according to the invention.

[0037] FIG. 2 is a diagram showing a process for extracting an active ingredient from horseradish to prepare a soil pest control composition having glucosinolate extracted from rapeseed meal and horseradish according to the invention.

[0038] Figure 3 is a table showing the density suppression effect of the rapeseed meal and horseradish mixed control agent according to the present invention against root-knot nematodes.

[0039] Figure 4 is a table summarizing the results of a stability test of a mixed pesticide of rapeseed meal and horseradish according to the present invention.

[0040] Figure 5 is a graph showing the sinigrin peak values ​​of the extract extracted according to the present invention relative to the standard.

[0041] The present invention will be described in more detail below by means of preferred embodiments. However, it goes without saying that the scope of the present invention is not limited thereto.

[0042] In this specification, embodiments are provided to ensure that the disclosure of the invention is complete and to fully inform those skilled in the art of the scope of the invention, and the scope of the invention is defined only by the claims. Accordingly, in some embodiments, well-known components, well-known operations, and well-known techniques are not specifically described to avoid the invention being interpreted ambiguously.

[0043] The terms used herein are for describing embodiments and are by no means intended to limit the invention. In this specification, the singular form includes the plural form unless specifically stated otherwise in the text. Additionally, components and operations referred to as "comprising (or comprising)" do not exclude the presence or addition of one or more other components and operations.

[0044] The terms used in the claims and specification are defined as described below unless otherwise specified. Additionally, if any term or symbol used in this specification is not defined as set forth below, it shall have its general meaning in the art.

[0045] Practice of the present invention involves the use of conventional techniques within the art of organic chemistry, molecular biology (including recombination techniques), microbiology, cell biology, biochemistry, and immunology.

[0046] As used in this specification and the appended claims, in the context of describing elements, particularly in the context of the claims, singular and similar designations shall be interpreted to include both singular and plural forms unless otherwise indicated in this specification or clearly contrary to the context. References to ranges of values ​​in this specification are intended merely to function as a shorthand method for individually designating each individual value within a range, including upper and lower limits of the range, unless otherwise indicated in this specification, and each individual value is included in this specification as individually cited in this specification. All methods described in this specification may be performed in any suitable order unless otherwise indicated in this specification or clearly contrary to the context.

[0047] The term “nematode” as used in this specification refers to the peanut root-knot nematode (Meloidogyne arenaria), carrot root-knot nematode (Meloidogyne hapla), sweet potato root-knot nematode (Meloidogyne incognita), and Javanica root-knot nematode (Meloidogyne javanica), and refers to soil pests that cause significant damage to eggplant, potato, chili pepper, carrot, watermelon, cucumber, tomato, pumpkin, etc.

[0048] As used herein, the term "glucosinolate" refers to a compound composed of progoitrin, sinigrin, gluconapin, glucobrassicanapin, glucocochlearin, glucoiberin, glucoraphanin, glucoerysolin, glucotropaeolin, gluconasturtiin, glucobrassicin, neoglucobrassicin, 4-hydroxyglucobrassicin, 4-methoxyglucobrassicin, etc., which, by the action of the enzyme myrosinase It refers to compounds that emit isothiocyanate (ITC), organic cyanides (CN), oxazolidinethione (OZT), and ionicthiocyanate (SCN-).

[0049] The soil pest control composition of the present invention, comprising glucosinolates extracted from rapeseed meal and horseradish as active ingredients, comprises extracting indicator components progoitrin, gluconapin, and 4-hydroxyglucobrassicin by performing extraction on dried rapeseed meal powder using ethanol and water as solvents at a temperature of room temperature to 70°C for 30 minutes to 3 days, preferably 3 hours, and extracting indicator components sinigrin, 4-hydroxyglucobrassicin, and gluconapin by performing extraction on a dried horseradish sample using ethanol and water at a temperature of room temperature to 70°C for 30 minutes to 3 days, preferably 3 hours, and mixing these two extracted components in a certain ratio, preferably by weight ratio of 1:5 to 5:1, more preferably 1:5. Get.

[0050] According to another embodiment of the present invention, the two extract components may be composed of a diluted solution composition diluted 10 times with zeolite, either individually or in combination. In the case of the zeolite diluted 10 times composition in this manner, it can be seen that the control rate reaches 71.6%, which demonstrates a control efficacy that is in no way inferior to that of general chemical fertilizers.

[0051] According to another embodiment of the present invention, the solvents ethanol and water are used in a ratio of 10 to 40 of 60% ethanol when used with dried rapeseed meal powder, and in a ratio of 10 to 40 of 60% ethanol when used with dried horseradish samples. It has been found that using 60% ethanol in different specific ratios for each extraction target is most ideal for the effective extraction of active ingredients.

[0052] In addition, according to another embodiment, a method for preparing a soil pest control composition having glucosinolate extracted from rapeseed meal and horseradish of the present invention as an active ingredient comprises: a step of grinding dried rapeseed meal powder; a step of performing stirring extraction or reflux extraction using the ground material as a solvent in 10 to 40 times the amount of 60% ethanol at room temperature to 70°C for 30 minutes to 3 days; a step of filtering the extract and performing continuous centrifugation; a step of concentrating the centrifuged material under reduced pressure to remove alcohol and water; and a step of freeze-drying the extract;

[0053] The method comprises the steps of: freeze-drying a dried horseradish sample; grinding the freeze-dried sample; performing reflux extraction of the ground sample using 60% ethanol as a solvent in a ratio of 10 to 40 at room temperature to 70°C for 30 minutes to 3 days; performing continuous centrifugation of the extract; concentrating the centrifuged material under reduced pressure to remove alcohol and water; and freeze-drying the extract.

[0054] The method may consist of a step of mixing each of the above freeze-dried extracts in a certain ratio.

[0055] According to another embodiment of the present invention, the mixing ratio of the rapeseed meal and the freeze-dried extract of horseradish may be mixed in a weight ratio of 1:5 to 5:1, preferably 1:1.

[0056] Each process for preparing a soil pest control composition having glucosinolate extracted from rapeseed meal and horseradish as an active ingredient according to the above-described invention is illustrated more specifically in FIG. 1 and FIG. 2, respectively.

[0057] Referring to FIG. 1, FIG. 1 is a drawing showing a process for extracting an active ingredient according to the present invention from rapeseed meal.

[0058] Also, referring to FIG. 2, FIG. 2 is a diagram showing a process for extracting an active ingredient according to the present invention from horseradish.

[0059] According to the process shown in Fig. 1, progoitrin, gluconapin, and 4-hydroxyglucobrassicin are efficiently extracted from rapeseed meal, and according to the process shown in Fig. 2, sinigrin, 4-hydroxyglucobrassicin, and gluconapin are efficiently extracted from horseradish.

[0060] The mixed control agent of rapeseed meal and horseradish extract according to the composition of the present invention has an excellent density suppression effect against root-knot nematodes and shows a synergistic effect in nematode control, and detailed data is shown in Fig. 3.

[0061] The present invention will be explained in more detail below by way of examples, but it is not intended that the present invention be limited to these examples. In addition, in the examples described below, unless specifically noted otherwise, the ratio of the composition is expressed as a weight ratio.

[0062] Example 1

[0063] Preparation of rapeseed meal extract

[0064] 5 kg of dried rapeseed meal powder was homogeneously ground in a grinder, and then 60% ethanol was added as a solvent in a 40-fold ratio to the obtained ground material and reflux extracted at 70°C for 3 hours. The reflux extract was filtered to remove the rapeseed meal residue, and the obtained filtrate was subjected to continuous centrifugation to obtain a higher purity.

[0065] The substance obtained by centrifugation was concentrated under reduced pressure to remove alcohol and water, and the extract was freeze-dried to obtain a dried rapeseed meal extract.

[0066] Example 2

[0067] Preparation of horseradish extract

[0068] 600g of dried horseradish sample was freeze-dried and then ground. The freeze-dried and ground sample was reflux-extracted using 60% ethanol as a solvent at 70°C for 3 hours at a volume of 40. Continuous centrifugation was performed on the reflux-extracted material, and the centrifuged substance was concentrated under reduced pressure to remove alcohol and water, and then freeze-dried to obtain a dried horseradish extract.

[0069] Example 3

[0070] The freeze-dried rapeseed meal extract and horseradish extract obtained in Examples 1 and 2 above were mixed in ratios of 1:5, 1:3, 1:1, 3:1, and 5:1, respectively, to obtain a soil pest control composition having glucosinolates extracted from rapeseed meal and horseradish as active ingredients.

[0071] The soil pest control effect and the effects on the natural environment and organisms of the compositions prepared according to each embodiment of the present invention were investigated, and the results are summarized in the following experimental examples.

[0072] Experimental Example 1

[0073] The density-inhibiting effect of the rapeseed meal and horseradish mixed control agent according to the present invention on root-knot nematodes was investigated and the results are shown in Figure 3.

[0074] Experimental Example 2

[0075] As a result of investigating the median lethal dose of the composition according to the present invention prepared according to Examples 1 to 3 above, it corresponded to Class IV (low toxicity).

[0076] In addition, based on the acute toxicity test results and classification according to pesticide toxicity and persistence levels, it was classified as Grade III (low toxicity).

[0077] In an ocular mucosal irritation test using New Zealand white rabbits, the composition according to the example was found to be a non-irritating substance, and in addition, in a skin irritation test of the composition using New Zealand white rabbits, it was classified as having no skin irritation.

[0078] Finally, in the acute contact toxicity test of the composition according to the example on honeybees (Apis mellifera), the 24 and 48-hour median lethal doses for honeybees were determined to be very stable, with values ​​exceeding 100,000 μg / honeybee.

[0079] The results of the above tests, including fish toxicity tests, are summarized in Figure 4.

[0080] In the above description, room temperature refers to 15 to 25 degrees Celsius.

[0081]

[0082] Foregoing, specific parts of the present invention have been described in detail. It will be apparent to those skilled in the art that such specific descriptions are merely preferred embodiments and do not limit the scope of the invention. Accordingly, the actual scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A composition for controlling soil pests comprising glucosinolates extracted from rapeseed meal and horseradish as active ingredients, characterized by being obtained by mixing two extracted components, wherein dried rapeseed meal powder is extracted in ethanol and water using a solvent at a temperature of room temperature to 70°C for 30 minutes to 3 days to extract the indicator components progoitrin, gluconapin, and 4-hydroxyglucobrassicin, and dried horseradish sample is extracted in ethanol and water at a temperature of room temperature to 70°C for 30 minutes to 3 days to extract the indicator component sinigrin.

2. A composition for controlling soil pests having glucosinolate extracted from rapeseed meal and horseradish as an active ingredient, characterized in that, in claim 1, the extract component is a diluted solution composition obtained by diluting 10 times with zeolite.

3. A composition for controlling soil pests having glucosinolate extracted from rapeseed meal and horseradish as an active ingredient, characterized in that, in claim 1, the solvents ethanol and water are each used in a ratio of 10 to 40 times 60% ethanol when used with dried rapeseed meal powder, and in a ratio of 10 to 40 times 60% ethanol when used with dried horseradish samples.

4. A composition for controlling soil pests having glucosinolates extracted from rapeseed meal and horseradish as active ingredients, characterized in that, in Claim 1, the rapeseed meal extract and the horseradish extract are mixed in a weight ratio of 1:5 to 5:

1.

5. Step of grinding dried rapeseed meal powder: A step of performing stirring extraction or reflux extraction using the ground material as a solvent in 10 to 40 times 60% ethanol at room temperature to 70°C for 30 minutes to 3 days: A step of filtering the above extract and performing continuous centrifugation; Step of removing alcohol and water by concentrating the centrifuged material under reduced pressure: and A step of freeze-drying the extract; Step of freeze-drying a dried horseradish sample; Step of grinding the freeze-dried sample; Step of performing reflux extraction of the ground sample using 60% ethanol as a solvent in 10 to 40 times the amount at room temperature to 70°C for 30 minutes to 3 days: A step of performing continuous centrifugation on the above extract; Step of removing alcohol and water by concentrating the centrifuged material under reduced pressure: and It consists of a freeze-drying step of the extract, A method for preparing a soil pest control composition having glucosinolate extracted from rapeseed meal and horseradish as an active ingredient, characterized by comprising the step of mixing the above-mentioned freeze-dried extracts in a fixed ratio.

6. A method for preparing a soil pest control composition having glucosinolate extracted from rapeseed meal and horseradish as an active ingredient, characterized in that, in claim 5, the freeze-dried extracts of rapeseed meal and horseradish are mixed in a weight ratio of 1:5 to 5:1.

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